Chloroacetyl chloride → Chloroacetic acid morpholine carboxamide

HRID 1451233

Reaktionsgleichung

Reaktionsgleichung von HRID 1451233
[Cl:1][CH2:2][C:3](Cl)=[O:4].C[N:7]1CC[O:10]CC1.[NH:13]1[CH2:18][CH2:17][O:16][CH2:15][CH2:14]1>ClCCl>[N:13]1([C:3]([NH2:7])=[O:4])[CH2:18][CH2:17][O:16][CH2:15][CH2:14]1.[Cl:1][CH2:2][C:3]([OH:4])=[O:10]

Komponenten

5

Versuchsvorschrift

Combine chloroacetyl chloride (2.00 mL, 25.0 mmol) and N-methylmorpholine (2.76 mL, 25.0 mmol) in dichloromethane (100 mL). Cool in an ice-bath. Add morpholine (2.19 mL, 25.0 mmol) and stir in the ice-bath for 1 hour. Warm to ambient temperature and stir for 1 hour. Extract with cold aqueous 5% sulfuric acid solution, saturated aqueous sodium bicarbonate solution, and saturated aqueous sodium chloride solution. Dry the organic layer over Na2SO4, filter, and evaporate in vacuo to obtain chloroacetic acid morpholine carboxamide.

Aufarbeitung

  1. temperatureCool in an ice-bath
  2. extractionExtract with cold aqueous 5% sulfuric acid solution, saturated aqueous sodium bicarbonate solution, and saturated aqueous sodium chloride solution
  3. dry with materialDry the organic layer over Na2SO4
  4. filtrationfilter
  5. customevaporate in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-517c578409644858ab5400bf7e45ff0a
Quelldatensatz
uspto-grants-1997_02
Patentnummer
US05604221

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